【商检行业标准(SN)】 出口粮谷中烯菌灵残留量检验方法

中华人民共和国进出口商品检验行业标准SN 05201996
出口粮谷中烯菌灵残留量检验方法Method for the determination of imazalilrcsidues in cercals for export1996-04-29发布
中华人民共和国国家进出口商品捡验局1996-10-01实施
SNC520.1996
本标准与根据/T1.11SS3长饿化工作小则务1毕元：标准的起克与整则第部分：标准编写的基不机定》及5V/TCC01一19954出二商品中衣母药饿留生及生物卡东控验方法标准编马的基太规实的要少而选行端写范：其中测定方法静国内外行关文献，丝研，改准和收证后而制定的，六标准同时制定了州样利制祥支法。滇定低限是根国际上对较苍中筛萨灵残胃量盘的效高吸些和到定方法约灵做度耐制定的对求A为提示控用录。
不标确止中件人舌儿国素连出山商品检验局接出并三门。本标准新单单位中人民共和雨上海进自高品控监局太标源主票起其人降家华，
1范围
中华人民共和国进出口商品捡验行业标准出口粮谷中烯菌灵残留量检验方法Method for the determlnatilon of Imazaluresidues in cereals for exportSN0520—1996
车标准规究「山口稳省中烯置灵氓留量控验差推样、制拦知俊相色谱测定方法。本标能道用于出口大米中烯或残留的检验2抽样和制样
2. 1验批
以不留过1000表（200+)为检验）同一检短排的前品应任相反的特作，妇色装，标记、产控，规格和等级等。2.2抽岸数孕接-非总拨数价平方限式（1取：AEYN
，V——全批教：
市样您。
法：值取整数小数分向前进节力整效，2.3一
2.3.1金厚首管改均器：全长55cm（包活于）,直径1.m：放长度应让径对线度的率：23.2取梯许。
2.3.3办详板。
2.3.4样鼎带（我可封。
2.3-5分律布或活斥消物.
2.2油栏方先
2.4.1倒包抽年
点理操的各部位能机抽求2.2鼠定的盘拍净件数*：18%（每批、般不少于范）将装口键线全部升，平肾十分栏市成：他消净的辅求物上，双于案尴载底两们提起约成们值拖1㎡以上使签内货物金部到出，越合货物的外观，气味，有元发减、变质等，并专老您内汇整问已质居存句，确议借沉后.开改础随机在各环取羊品，将样品需入盛样器内。发放致样品装口减基本致。
2.4.2袋内抽革
按2.2规定的应拼拦袋数的杀，在准练四用上，中，下卒层以曲线形走向随机轴取，决取挡骼2.3.等增朝下，从每等一角依斜对角与向入教内，能后将管持负只期上，计启取样器，立助将样品人样容器成，每蒙抽取件品数收应与2.4.来本致每批样品总量成不少kg
中华人民共和国国家进出L商品检验局196-14-29批准1996-10-01实施
2.4.3大缩分
SV 0520-.1946
东中袋内和到包润拉所坂全部推.倒于分样布上，用分样板按四分法销分山栏完不少于2kg，盛予样品简闪，加款正快顺标记并及时避交实烩室2.5试样！备
将择需接国分法靠分至「k，全部唇碎准适过与筛，混与，均分成两份京单，表入治净的容器内，密势.核归标，
2.E试样保存
试样于一5以下送长存
注，车抽性和两样的投作过中，必罚花止样巧完州划来成发牛使密构含互的变化，3测定方法
3.1方达差要
以之酸乙酪绿取样品中的烯灵，希聚友扰成，酸或化气升之袋/嘴提收，蒸六乙胺乙酯残渣落解于流动相：配有费整划露的液程免牌没测定，外标法定量3-2料
除习有规定外，试马分折纯，术火燃循水。3-2.1乙乙能：。
3.2.2乙：燃外光谱级，
3.2.3航双：优线纯，约1.1g/m。3.2.4硫求落液..1rl/L
3.2.5氢氧化钠溶液：1l/L
3.2.6碳装销落液：5%（m/。
3.2.7磷酸热级准带，分.称取0.2mal/.样双二点销68ml0.2u./辨般氢.二钠32ml混勺，H调至7.5，移取Jm鼠于1容口中,新入ml/氧化钠落载2mL,混询用水定容单刻虑,3.2.B无碳题销：630灼烧41含却后于闭容露中备用：3.2.9尚标痛品纯度，
3.2.1惯菌灵标准溶激，准确你欣造单的需灵标品，用中品制比液度为[00必的乐降能各拨，根据需要移报适量堵餐液.用效气将甲醇吹去片用流动剂配门或造当浓废的标准工作落够，3.3仅器和该备
3.3.1激托诺仅系1案等抢测器
3.3.2 质3 ) r/。
3.33离.0/nn
3.3.4施转蒸发器
3.3.5做量造针器：2h、-03l..
3.4测定步案
3.4.1提璨化
取试推约&（种确至1，产小ml心势中.加入2无水流度的、25之能乙能均质2-离心1M/r）将上消液格入125分液通斗十，践盗用25mL己乙商安三述操作重复处理次合并上湾索于皱满牛中，用M，碳酸期势液烘录之融艺醇列，开么低酸钢洗液乐20m.然增水满<.醛/前指.弃六水料、（波带档分划片20、15mL函酸路题：0.12el/L提最，合并硫酸机弃去乙致乙虚杆。用乙较之醛洗统胶召，办去酸乙酯推，日1mal.率化液减化酸潜液（药1m1.)后，月×5m：.乙酸乙的提取.台并乙酸乙将析.并经元水硫载钳脱水，收出于梨形瓶中.求浴0：的施转杰发器上索发至逆一准确加入1mT.须相3.4.2.1r)以率解感经045m德英过滤后供液护色潜潮定，3.4.2测定
3.4.2.1微色谱杀牛
SN0520-1996
a）色谱住：府加正生Z-inodulBordapuku.10cmXmm(a）粹1kmb）格汇器UV+204m：
心流实相乙膜磁最盐频冲波（11：d）洗污：2ml./min
e）色谱柱温度：空湿
3.4.2.2没相长谱测定
根据详中烯菌录公量情况，选定峰相近的标消工作伊被标准工作筛流求样滤中烯谜灵节响高恒均应在仪器的检测要必范问内，对标准上作辫接样激等本积参插成样测定。在上违垒落茶件下烯的灵为保留时间约为净min。标准品色谱图见附录A中图Al：3.4.3空当试验
除不加试均方~，均投上述测定求骤进行。3.5随果计算可最述
用色恶效据处理机成式(2计并试栏士烯菌灵残酉x=
我，x
试悼中菌烫线留量，mg/kg;
液娣菌灵色呼高-mra
标准T.件将液宁烯荣的色谱蜂高，mTL:标滑作率液中稀菊浓度.
控液量终亲客体积，ml；
最终样液济代表药成样量·品。注，计弹站器如除实白值，
测定低限.回收率
4.1测定限
本达的谢定假限为0.5
4. 2放点
回收室的实验数据：
筛函灵策度在0.025mg/kg时，2收率为S4.；烯速灵率兜在0.5mg/kg，可收01.0%离英浓度在1.1 mg/kg对，可收率为 9.1X。(2）
SN 05201996
（提示的附）
标准品色请图
缔天兰园
SY3520-1996
Foreword
This luelarid wes draded in acptrdancc with the Ieiquiremnta of GB/T I. -\ Isy'LircetivrgiThe main tirafter nf this atandard is Chen JiehceNnrr- I'fis Pingisa veraion.n Tvg.ala ion Jror, the Chr.oeae lexl,is solely bor Hwidur.ze.Prufessional Standard uf the Peeple's Repuhlic of ChinaFor Impnrt aud Export Comnrdity InspectionMcthod for thc determination of Imazaliresidues in cereals for exportSupe
SN0520
This starwdard s[xx:fiex Ile ruthuxd, of siruling, ple prepa:ation and dctermrinatun of imizali]-sidurs hy lingi:l chrmatograihay in cereals tor exrt.This standart ts apphiesEe io she dcrerncineror, of mazalil resiklue content in rice far exreort.2Samplingand samplepreparatloa2.1Ir.spectior. Int
Each napecion lor shomld not exeecd 4oo hars (20o t)The chari ereris-it rf -r carg wiihin ilhe i,ar, iusjwrlin lut sueh us cking smark rorigir. rgpcifica-Tisn.grade cte. asl.cule be the sanr.c.2. 2 Quantity f zample -skenThe aas:ber uf beg lu l: sumi:lrd sh.ill be raleull.aul aceurding to the formula iola rt.ruer r.[ aag irs t
a..nun:ber ct bag to be zanpled.Note : L! vsiue a is ipitin dnciroaitoimd art rae cecirai pertrwhich i addej az urui:y xo llie izlleged. palz ul a2. 3Supling ole
2. 3. 1Meazllie sanpler : Lergth (including handle) : 55 m: diamcter:1. 5, cn. rgroave lenpth : lor.ger lhanhalf ihe d:agnnal lenyth ai the Lbag.2- 3- 2 Seinmlig atvr. .
2. 3. 3Plate for y.jarteruug.2. 3. 4 Suin?ie cantbag?,wajrh tan he sealed.2. 3. 5:lorh (or ntaer suitable material) shcet ,Fnr sempl: dividing (quarzcring)2. 4Smp:li-1g 1rix:-ilure
2. 4, :Sarapling by cruptyng sutD-aw 10 pe:cea: of the nur.ber nf bags specified in 2. 2 (nct les: tkan s bagei ar ary Fatt of the p:hat taludor. L.useatt anal ugpu ihu huigarurl lny it un u ilsin lath snl (ur ulhe: cleul sheri). Grt.sp tightIyr cnrners nf the hag, bnezrm enc raisc up to an angle of -s'll:g hackward fns ca 1 m unil all axnleni ntApproved by tke Shate Arlninistralion arInport ard Export Camnindity Iaspeclint ofthe People's Republk of China onApr.29,1996
Tmplemeated tronr Cra, 1.1996SN0570-1996
the bag :s enipried out, Chuck thn appearanae.odeur of :be gnods ar.d wlherker the konds are uoldy,rittcinzte. Alsa check prl.piqur ihr iguality of the gode sa uniform within and betweeu rhe haga. Aiter eonfirmangIhp ku-l., a int nnrmen. condition, acnop up tha sumple from different perta of the uut pouredl cum'tnt vi-ha shavel,and placa in a sample curuiner prrupsty. The ijuantiny sf rhe aa.apln drawn [roix each bag shonildbe basically ihe satr.c.
2.4.2Sumpli:g For ile ce:gals in the bagIriaw the Sanples fron B0 pxrcene of the nuntbur of bags syeeitisd in 2. 2 nu fullows: Alerg tau sincwave of tlue pile,craw 3amplea frumn ths buge of ilr pper,niduile ancl l:wpr pulls n: itie pilr :' ranclo'n. la.e:t th sansple:(2, 3, I),with its xroave [acinp dowawn:d,diagunaly inta cach bag.the su:n tae samplcrby 1giy'.druw min 1ha zampler.proreptly Four the aamaple inco & cortrircz. The quantity oi the sanpleriawn frmm eachs bag anall be bunca.ly the suree ai- in 2. 4. i.The iutal wcight ef che reprhrulalive nu-r:spln of weih, Im ahrald he rrl len, cl.a : ky.2. 4. 3 Recue-r1 uf grw xi.np.cPuir ill ili* sumplas (from both 2. 4. 1 and u. 4. 2)on a clean shce:+rcdi:ce to not leau than 2 kg w:th plaie hy quarcering. ['lace in a amp'e contziner,wead,label ul nprul to th lnhoratary r lire.2. 5I'-eparstion f trst saruplrRedac- the in-1.jil- Iu t 1 sg hy nuarter.eg-grind -aoroughly i:nc. Jet pas3 brouigh a 23-mest: sieve,rrix ilurougl.ly ard divide into 2 ecual porl:on3relacc in claan containcra,5oal and abcl.2. 6 Storegc of te1 g9mple
Tlw Test gemp'e shall be su>w-l Ielhrw (i' ard kcpt away from light.Nc.e: In the =re of xamping ard aemNc peeparntir?.jisrnutirn muasr u -witer in .wnid r r.min.rr. r:ry 'nn-s:he1 :pay =auae the tangc cd essid Je rnr tcat. Method or determinatka
3.Trincipke
he imazal] readuca r. rier Ar txiri\tel win ilyl arrlae.the txli is Ayain ha'-tted wih aridsalurior. be liquid ixurli;igrsirg- Tl:e acid phate is alkalified and extructec with ethyl acetate, Exgel the ethylt rrralt., lisrulve che residue in the mobile 2hie, rihe salcion ig analyzed by HPLC w:ch ultraviolet detcrsnr,using extemul sianriatrd method.3.2 Keagenrs and materiuls
=lr:tss utb-r: wiar fpw ified,the reagents should be zrn.ytically pure,\watex\ia ciglilled water.3.2.1Fihal Acctate:Redisti.lexl.3-2.2Aretortslr:UV grade.
3. ? 3 Sulfrc wd.ea [.&4 g-l 3. 2. 4Sulf-i: anid sn.tinr.. Aqucnus erlutinn. 3. 1 mo.,/L3.2.5Sxlinim hydrax:de olution Ayueoux rolurion,1 mol/t..3-2.6Sdium cazhanare solut:on,Aquxus solutiort.h!mcthyl uleohusl arul aepura n sulusius uf uo ug/nL in conentratian ag the standard atoek solutioa. Ac-crrding n the renuirenucnt pipet rersin amopr.1 l siandard arxk xolnlicr ,url prepare i: stuadzrd wurkingsolution of approptiale concentrarion wi:h the mab:le ptaze atter removal of neihyl alcohnl hy a cil:grncurrcrt.
3. 3Appsratas and enuigmenl免费标准下载网bzxz
3. 3. 1High pcrformance ligu:d -hroruatugraph,equipped ith IJV rietecy.3. 3. ? Hemogenicr r& 3 :/ms.3.3-3C-ul[ugu;5 U) r/min.
3. 3.4Rr.tary eveparanr.
3.3.5.Micro-syringe.25 ul.:100 pL3.4Procedure
3.4. 1 Extrge1irn and cleanupWeigh ra 5 g ef the iesr sample(aceurale 0. 1 ghintp u 5D nl. centrifuge tube,add 2 e rf amlydrrmiodiun sulfeic &ad 23 mL of cthyl acetare. Afcer homogenizing for 2 min And cecarifaging for I min(5 000[/sui-.lianeler ie nuperualain inli, 125 re.L ouxrulirg f, rnc.. Re[xut :hc operetieon or. the ragidue bsadding anuther 25i ml, of etbyl acctate, Canbine the 5iperneta:1 layeia n iha slr Hrlarating fer.. :sl:he er.hgl accrate phage witll zc ml, of sowinm raronale solurioa.and cizcard the ecdium cerborare washings, Wesh the ethyl arctale uhase cgrir. with 20 aL of weter,d:scnrd the equeou waahings. Extruc: theFthyl acetatc phase with successive 23 ml.,10 cal, nf gulfurir au:il iliem(o. - mul/L.), Ckruhicu thc sulfuric acic ex.racts.ard diacard thie ethyl cetare ehase. Wssh ihe safuuic arid extraet with 10 ral. rl ethyl ac-ctte und diseard thc ertyl ecerete washirgs, Alkalify the agucous rolutuon with i mol/L sod:um hydroxidesnl.l rn (ra 10 Jul.s. Fx1ra tlr Mjueruk m'sliun. Iwrt linps with S rnl, uf etltyl ueta curh, Combine thct.ay. Hcetate extract and let [ass throLgt. anhydrous sciur. stliate inzn pca-sbaped f.ask. F.viaeo-lle iirexiract acarly to drymeas on rorary avagnrarnt at 5o't:, L)isaolve ths residue in 1 ml. mobile phasc(3l. 4. 2.le>eulat:n, Fi,ter witli u, 45 rem silru,the nulaisn :s ready for ligsid chrumaarographic dcrerminalion.3.4.2Det-nrinalion
3. d.2. 1LC: operatiag coditiunE) LC column:Z mudlrl Bendapak CJC cmX8 mm(id).10 μrn(particle size);a) Detecor,TJV,204 nEaf
t) Mobile phase:Acetonitrile ptosphae butter syrianf1-1)d: Flow rete.2 ml./min;
+.) Cod..i. 1ernponr:-dt.re : Rixr.3. 4. 2. 2 1.C. determinatior..trx.r! s
Acrording zo the approxinzte coricerilratior. o: inazilil in -he saple sa.utin, sc.cct the staniardviurking so.utior. wich sitnilur ueck height to that pf the aemple solut:en. The responses af irnazalil ir. thestandarid woking sat.lion and sunple ssltirn xEiulri . wilna, tluu linrt: rrt.gu of the islin:encul dctee--iu. The star:da:d workirg solution xhuld se randoraly injected in-hetwcen xhe injrctint.s af the xrplr n:>lLcion uf cqual vnlimc. Lncer the abave cperating condition.the retentian -:me o irhazali is ca min. Fu11.i- i:hkirialigtr of hr slimrlar:l.st. fig- A ira Linux A3. 4. 3 3a test
'The operation of the blank rest i The aarre us th:a: described in the methud of determinatican hit wizinthe ouaissiur. ef sample L.tidition.3. 5Cadcnlalirr: arl +xp-rrssicr: uf :a: rennl8
SN0520
Ct.kulate tle iurden uf imalkli! renicluen in ihr Irsi irple by I.C ilala prixrr[orra.ija (?):
the reaidue cmtent of imazail in the test szmg:e.mg/kg:Aihe peak heigh: of irurralil tr. the saraple solutior ,ram?A,the pcek aicigh: uf ittuzalil ir: the xlinurdar:l wrurking x,lution,rm;the crneuatrationt uf iuruzalil ir:ttu luurdurl wr.rking w.lutior..pg/taL;ihe [.rs. volume o: the saly.ple salutinn .ml..the ucrreeponling niass of the teat sample r the fira. manpla solurian-g.Note : The bla nk vale xhouid be subtrzeted fram -he zbowe rusult us cakeulaion4 LImh f deierndnatdon and reovery4.1 TLimit of ceterminatiot.Th: limin of delergigation of this aierhod is G. 323 mg/kg4.2Rcewery
riuurdingto the
Araxi-rding Ii The x[erimenial dat:a.tle Inrifyint, rncen:satinne cf iniaaalil and ihil tor-asprneliugrccweniesare:
5. 025 mx/ka,the reeuvery 54.3/. 05u ng/kg.:hr rr.very 1ri. 0%:1. 00 mg/sg:the recsvery $1. 5.1
SN 0520
AnmerA
(i-lisrmar.ve)
Chromnaiogram or the standerdFia. AJ Chrrratogrt of 1he ien.alil kirulard
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